CN114031118A - Preparation method of high-purity alpha-zirconium tungstate - Google Patents
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Abstract
A preparation method of high-purity alpha-zirconium tungstate, relating to a preparation method of a negative expansion material zirconium tungstate. The method aims to solve the problems of low purity, easy decomposition and crystal water inclusion in the existing zirconium tungstate preparation method. The method comprises the following steps: weighing WO3And ZrO2The raw materials are ball-milled to obtain primary mixed powder; primary sintering of the mixed powder, namely primary sintering of the primary mixed powder into a block and water quenching; adding the primary mixed powder after crushing to obtain secondary mixed powder, and sintering, crushing and drying the secondary mixed powder to obtain zirconium tungstate powder; the invention passes through reasonable WO3And ZrO2In a molar ratio of (A), adding an excess of WO3And using WO by secondary sintering3The residual ZrO2Conversion to zirconium tungstate to avoid ZrO2Remains, improves ZrO2Conversion rate; twice sintering and quenching are carried out to remove ZrO2And the grain size increase of the zirconium tungstate and the generation of the gamma-zirconium tungstate caused by multiple sintering are avoided.
Description
Technical Field
The invention relates to a negative expansion material alpha-ZrW2O8The preparation method of (1).
Background
Most solid materials can expand with heat and contract with cold when the ambient temperature changes, and the volume of some materials can contract with the temperature rise, so that a negative expansion effect is presented. Zirconium tungstate (ZrW)2O8) The material has a negative thermal expansion coefficient, and has the same negative expansion effect in a large temperature range of 0.3-1050K. ZrW2O8Cubic phase alpha-ZrW exists at low temperature2O8And quadrature phase gamma-ZrW2O8The coefficients of expansion are respectively-8.7X 10-6K-1and-1X 10-6K-1。α-ZrW2O8The negative expansion effect is more obvious, and the material with the positive thermal expansion coefficient is added to effectively adjust the thermal expansion coefficient, so that the material is applied to industries such as precision instruments, optical devices and the like.
α-ZrW2O8The preparation and synthesis method of (A) can be mainly divided into a wet method and a dry method. The wet method mainly comprises a sol-gel method, a hydrothermal method, a coprecipitation method and the like. However, alpha-ZrW prepared by a wet process2O8Crystal water is inevitably included so that alpha-ZrW2O8The application is greatly limited. In addition, the liquid phase method has complex process and high cost, and a large amount of waste liquid and waste gas are generated in the preparation process, so that the environment is seriously polluted, and the method has great limitation.
Traditional dry method for preparing alpha-ZrW2O8Due to WO3Or ZrO2Residual and presence of gamma-ZrW2O8And the like, and also has disadvantages of low purity and easy decomposition. Therefore, the low-cost high-purity negative expansion material alpha-ZrW is urgently needed2O8The preparation method of (1).
Disclosure of Invention
The invention aims to solve the problem of the existing alpha-ZrW2O8The preparation method has the problems of low purity, easy decomposition and crystal water inclusion, and provides the high-purity alpha-ZrW2O8The preparation method of (1).
The invention relates to high-purity alpha-ZrW2O8The preparation method comprises the following steps:
firstly, preparing mixed powder
Weighing WO3And ZrO2The raw materials are ball-milled to obtain primary mixed powder;
said WO3And ZrO2The molar ratio is (2.0-2.2): 1;
the ball milling adopts wet ball milling, absolute ethyl alcohol with the volume of 0.1-30% of the primary mixed powder is added, the ball-material ratio is (5-20):1, the rotation speed is 100-;
secondly, primary sintering of the mixed powder
Uniformly filling the primary mixed powder obtained in the step one in a crucible, sintering, and then cooling to room temperature to obtain a primary sintered block;
the sintering temperature is 1150-1260 ℃, and the time is 5 min-6 h;
the cooling mode is water quenching;
crushing of once sintered block
Crushing the primary sintered block obtained by sintering in the step two to be less than 200 mu m, and drying to obtain crushed powder;
the crushing is carried out by adopting a high-energy ball milling or grinding mode;
fourthly, mixing the crushed powder and the raw material mixed powder
Weighing the primary mixed powder prepared in the step one, and mixing the primary mixed powder with the crushed powder obtained in the step three to obtain secondary mixed powder;
the mass ratio of the primary mixed powder to the crushed powder is (0.1-0.3) to 1;
the mixing method is wet ball milling, and 0-30% volume of absolute ethyl alcohol of secondary mixed powder is added, wherein the ball-material ratio is (5-20):1, the rotating speed is 50-200rpm, and the time is 1-3 h;
five, two times sintering
Uniformly filling the secondary mixed powder obtained in the step four in a crucible, sintering, cooling to room temperature to obtain a secondary sintered block, crushing and drying the sintered block to obtain ZrW2O8Powder;
the sintering temperature is 1150-1260 ℃, and the time is 5 min-6 h;
the cooling mode is water quenching.
The invention has the following beneficial effects:
1. preparation of alpha-ZrW by existing solid phase sintering2O8In the process, due to WO3Has a relatively low vapor pressure and sublimes during the temperature rise, leaving residual ZrO in the sintered product2. The invention reasonably selects the raw material WO3And ZrO2By adding an excess of WO3And using WO in a secondary sintering manner3The residual ZrO2Conversion to ZrW2O8Avoid ZrO2Remains, improves ZrO2Conversion rate; meanwhile, the long-time heat preservation in the secondary sintering can be realized by WO3Removing WO excessively added3Further improves the alpha-ZrW2O8The purity of (2). The invention realizes the removal of ZrO by only carrying out twice sintering and quenching2Avoid the ZrW caused by multiple sintering2O8And the product tends to be dense, resulting in gamma-ZrW2O8And (4) generating.
2、ZrW2O8Metastable at room temperature to 777 ℃ and destabilizing decomposition begins to occur at 777 ℃ until 1105 ℃. The sintering temperature is 1150-1260 ℃, quenching is adopted for rapid cooling, and ZrW is arranged in the temperature range2O8Stable structure and capability of avoiding forming amorphous ZrW2O8And avoid ZrW2O8Destabilizing and decomposing, and ensuring the purity.
3. The invention provides a method for quickly and efficiently preparing alpha-ZrW2O8In the manner of (a) or (b),simple process, alpha-ZrW2O8High purity and easy realization of industrialized production and application.
Drawings
FIG. 1 is an SEM image of zirconium tungstate prepared in example 1;
fig. 2 is an XRD pattern of zirconium tungstate prepared in example 1.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
The first embodiment is as follows: the high purity α -ZrW of this embodiment2O8The preparation method comprises the following steps:
firstly, preparing mixed powder
Weighing WO3And ZrO2The raw materials are ball-milled to obtain primary mixed powder;
said WO3And ZrO2The molar ratio is (2.0-2.2): 1;
secondly, primary sintering of the mixed powder
Uniformly filling the primary mixed powder obtained in the step one in a crucible, sintering, and then cooling to room temperature to obtain a primary sintered block;
the sintering temperature is 1150-1260 ℃, and the time is 5 min-6 h;
the cooling mode is water quenching;
crushing of once sintered block
Crushing the primary sintered block obtained by sintering in the step two to be less than 200 mu m, and drying to obtain crushed powder;
fourthly, mixing the crushed powder and the raw material mixed powder
Weighing the primary mixed powder prepared in the step one, and mixing the primary mixed powder with the crushed powder obtained in the step three to obtain secondary mixed powder;
the mass ratio of the primary mixed powder to the crushed powder is (0.1-0.3) to 1;
the mixing method is wet ball milling, and 0-30% volume of absolute ethyl alcohol of secondary mixed powder is added, wherein the ball-material ratio is (5-20):1, the rotating speed is 50-200rpm, and the time is 1-3 h;
five, two times sintering
Uniformly filling the secondary mixed powder obtained in the step four in a crucible, sintering, cooling to room temperature to obtain a secondary sintered block, crushing and drying the sintered block to obtain ZrW2O8Powder;
the sintering temperature is 1150-1260 ℃, and the time is 5 min-6 h;
the cooling mode is water quenching.
The embodiment has the following beneficial effects:
1. preparation of alpha-ZrW by existing solid phase sintering2O8In the process, due to WO3Has a relatively low vapor pressure and sublimes during the temperature rise, leaving residual ZrO in the sintered product2. The embodiment reasonably selects the raw material WO3And ZrO2By adding an excess of WO3And using WO in a secondary sintering manner3The residual ZrO2Conversion to ZrW2O8Avoid ZrO2Remains, improves ZrO2Conversion rate; meanwhile, the long-time heat preservation in the secondary sintering can be realized by WO3Removing WO excessively added3Further improves the alpha-ZrW2O8The purity of (2). The embodiment realizes ZrO removal by only performing sintering and quenching twice2Avoid the ZrW caused by multiple sintering2O8And the product tends to be dense, resulting in gamma-ZrW2O8And (4) generating.
2、ZrW2O8Metastable at room temperature to 777 ℃ and destabilizing decomposition begins to occur at 777 ℃ until 1105 ℃. The sintering temperature of the embodiment is 1150-1260 ℃, quenching is adopted for rapid cooling, and ZrW is arranged in the temperature range2O8Stable structure and capability of avoiding forming amorphous ZrW2O8And avoid ZrW2O8Destabilizing and decomposing, and ensuring the purity.
3. This embodiment provides a speedyEfficient preparation of alpha-ZrW2O8The method has simple process and alpha-ZrW2O8High purity and easy realization of industrialized production and application.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: step one of the WO3And ZrO2The molar ratio is 2.0: 1.
the third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and step one, ball milling is carried out by adopting a wet ball milling method, absolute ethyl alcohol with the volume of 10 percent of that of the primary mixed powder is added, the ball-material ratio is (5-20):1, the rotating speed is 100-250rpm, and the time is 1-3 h.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and step one, ball milling is carried out by adopting a wet ball milling method, absolute ethyl alcohol with the volume of 10 percent of that of the primary mixed powder is added, the ball-material ratio is 10:1, the rotating speed is 100-250rpm, and the time is 1-3 h.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and step one, ball milling is carried out by adopting a wet ball milling method, absolute ethyl alcohol with the volume of 10 percent of that of the primary mixed powder is added, the ball-material ratio is (5-20):1, the rotating speed is 200rpm, and the time is 1-3 h.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and the sintering temperature in the second step is 1170 ℃ for 5 min-6 h.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and step three, crushing by adopting a high-energy ball milling or grinding mode.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and fourthly, the mass ratio of the primary mixed powder to the crushed powder is 0.2: 1.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and step four, performing wet ball milling, adding 0-30 vol% of absolute ethyl alcohol into the secondary mixed powder, wherein the ball-material ratio is 10:1, the rotating speed is 100rpm, and the time is 1-3 h.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: and fourthly, the sintering temperature is 1170 ℃ and the time is 5 min-6 h.
Example 1:
this example is a high purity alpha-ZrW2O8The preparation method comprises the following steps:
firstly, preparing mixed powder
Weighing WO3And ZrO2The raw materials are ball-milled to obtain primary mixed powder;
said WO3And ZrO2The molar ratio is 2.15: 1;
the ball milling adopts wet ball milling, 20 volume percent of absolute ethyl alcohol of primary mixed powder is added, the ball-material ratio is 15:1, the rotating speed is 200rpm, and the time is 3 hours;
secondly, primary sintering of the mixed powder
Uniformly filling the primary mixed powder obtained in the step one in a crucible, sintering, and then cooling to room temperature to obtain a primary sintered block;
the sintering temperature is 1170 ℃ and the time is 45 min;
the cooling mode is water quenching;
crushing of once sintered block
Crushing the primary sintered block obtained by sintering in the step two to be less than 200 mu m, and drying to obtain crushed powder;
the crushing is carried out by adopting a high-energy ball milling mode;
fourthly, mixing the crushed powder and the raw material mixed powder
Weighing the primary mixed powder prepared in the step one, and mixing the primary mixed powder with the crushed powder obtained in the step three to obtain secondary mixed powder;
the mass ratio of the primary mixed powder to the crushed powder is 0.15: 1;
the mixing method is wet ball milling, and 20% volume of absolute ethyl alcohol of secondary mixed powder is added, the ball-material ratio is 10:1, the rotating speed is 50rpm, and the time is 1 h;
five, two times sintering
Uniformly filling the secondary mixed powder obtained in the step four in a crucible, sintering, cooling to room temperature to obtain a secondary sintered block, crushing and drying the sintered block to obtain ZrW2O8Powder;
the sintering temperature is 1170 ℃ and the time is 40 min;
the cooling mode is water quenching.
Fig. 1 is an SEM image of zirconium tungstate prepared in example 1. FIG. 2 is an XRD pattern of zirconium tungstate prepared in example 1; as can be seen from FIG. 2, all of the α -ZrW obtained in example 12O8Absence of gamma-ZrW 2O8, WO3And ZrO2. In the embodiment, raw materials WO are reasonably selected3And ZrO2By adding an excess of WO3And using WO in a secondary sintering manner3The residual ZrO2Conversion to ZrW2O8Avoid ZrO2Remains, improves ZrO2Conversion rate; meanwhile, the long-time heat preservation in the secondary sintering can be realized by WO3Removing WO excessively added3Further improves the alpha-ZrW2O8The purity of (2). In this example, ZrO removal was achieved by performing sintering and quenching only twice2Avoid the ZrW caused by multiple sintering2O8And the product tends to be dense, resulting in gamma-ZrW2O8And (4) generating. In the embodiment, the sintering temperature is 1150-1260 ℃, quenching is adopted for rapid cooling, and ZrW is arranged in the temperature range2O8Stable structure and capability of avoiding forming amorphous ZrW2O8And avoid ZrW2O8Destabilizing and decomposing, and ensuring the purity. This example provides a method for preparing α -ZrW rapidly and efficiently2O8The method has simple process and alpha-ZrW2O8High purity and easy realization of industrialized production and application.
Claims (10)
1. High-purity alpha-ZrW2O8The preparation method is characterized by comprising the following steps: high-purity alpha-ZrW2O8The preparation method is as followsThe method comprises the following steps:
firstly, preparing mixed powder
Weighing WO3And ZrO2The raw materials are ball-milled to obtain primary mixed powder;
said WO3And ZrO2The molar ratio is (2.0-2.2): 1;
secondly, primary sintering of the mixed powder
Uniformly filling the primary mixed powder obtained in the step one in a crucible, sintering, and then cooling to room temperature to obtain a primary sintered block;
the sintering temperature is 1150-1260 ℃, and the time is 5 min-6 h;
the cooling mode is water quenching;
crushing of once sintered block
Crushing the primary sintered block obtained by sintering in the step two to be less than 200 mu m, and drying to obtain crushed powder;
fourthly, mixing the crushed powder and the raw material mixed powder
Weighing the primary mixed powder prepared in the step one, and mixing the primary mixed powder with the crushed powder obtained in the step three to obtain secondary mixed powder;
the mass ratio of the primary mixed powder to the crushed powder is (0.1-0.3) to 1;
the mixing method is wet ball milling, and 0-30% volume of absolute ethyl alcohol of secondary mixed powder is added, wherein the ball-material ratio is (5-20):1, the rotating speed is 50-200rpm, and the time is 1-3 h;
five, two times sintering
Uniformly filling the secondary mixed powder obtained in the step four in a crucible, sintering, cooling to room temperature to obtain a secondary sintered block, crushing and drying the sintered block to obtain ZrW2O8Powder;
the sintering temperature is 1150-1260 ℃, and the time is 5 min-6 h;
the cooling mode is water quenching.
2. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: step (ii) ofOne said WO3And ZrO2The molar ratio is 2.0: 1.
3. high purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: and step one, ball milling is carried out by adopting a wet ball milling method, absolute ethyl alcohol with the volume of 10 percent of that of the primary mixed powder is added, the ball-material ratio is (5-20):1, the rotating speed is 100-250rpm, and the time is 1-3 h.
4. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: and step one, ball milling is carried out by adopting a wet ball milling method, absolute ethyl alcohol with the volume of 10 percent of that of the primary mixed powder is added, the ball-material ratio is 10:1, the rotating speed is 100-250rpm, and the time is 1-3 h.
5. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: and step one, ball milling is carried out by adopting a wet ball milling method, absolute ethyl alcohol with the volume of 10 percent of that of the primary mixed powder is added, the ball-material ratio is (5-20):1, the rotating speed is 200rpm, and the time is 1-3 h.
6. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: and the sintering temperature in the second step is 1170 ℃ for 5 min-6 h.
7. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: and step three, crushing by adopting a high-energy ball milling or grinding mode.
8. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: and fourthly, the mass ratio of the primary mixed powder to the crushed powder is 0.2: 1.
9. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: step (ii) ofAnd fourthly, performing wet ball milling, adding 0-30 vol% of absolute ethyl alcohol of the secondary mixed powder, wherein the ball-material ratio is 10:1, the rotating speed is 100rpm, and the time is 1-3 h.
10. High purity α -ZrW according to claim 12O8The preparation method is characterized by comprising the following steps: and fourthly, the sintering temperature is 1170 ℃ and the time is 5 min-6 h.
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